高效液相色谱法测定冰鲜海产品中的甲醛

Determination of formaldehyde in iced fresh seafood by high performance liquid chromatography

目的建立高效液相色谱法测定冰鲜海产品中甲醛含量的方法。方法冰鲜海产品中的甲醛与2,4-二硝基苯肼-乙酸钠缓冲溶液衍生反应得到甲醛-2,4-二硝基苯腙化合物,经过色谱柱SunFire C18(250 mm×4.6 mm,5μm)分离,以乙腈-水(50􀏑50,V/V)为流动相进行等度洗脱,柱温:30℃,流速:1.0 ml/min,二极管阵列检测器检测,检测波长为354 nm,外标法定量。结果甲醛衍生物在0 mg/L~2.0 mg/L呈良好的线性关系,相关系数(r)>0.999,在添加水平为1.0 mg/kg、5.0 mg/kg、10.0 mg/kg时,方法的平均加标回收率为75.4%~101.0%,相对标准偏差(RSD)为5.5%~7.9%,方法的检出限为0.3 mg/kg,稳定性满足实验要求。采用此方法对12份冰鲜海产品进行了分析,其中4份龙头鱼中均有检出,含量在3.19 mg/kg~11.6 mg/kg。结论该方法操作简便,准确率高,适用于冰鲜海产品中甲醛的快速检测。

Objective The high performance liquid chromatography method was developed for the determination of formaldehyde content in iced fresh seafood.Methods Formaldehyde in iced fresh seafood was derived from 2,4-dinitrobenzenehydrazine-sodium acetate buffer solution to formaldehyde-2,4-dinitrobenzenehydrazone,which was separated by a SunFire C18 column(250 mm×4.6 mm,5μm),with acetonitrile-water(50􀏑50,V/V)as the mobile phase,the column temperature was 30℃,the flow rate was 1.0 ml/min.The analytes were detected with PDAD detector at detection wavelength of 354 nm.The quantification was based on external standard method.Results Formaldehyde derivative had good linear relationships in the concentration of 0 mg/L-2.0 mg/L,and the correlation coefficient(r)was above 0.999.At the addition levels of 1.0 mg/kg,5.0 mg/kg and 10.0 mg/kg,the average recoveries were 75.4%-101.0%,and the RSD value was within 5.5%-7.9%.The limit of detection was 0.3 mg/kg.The method can be used for the qualitative and quantitative of formaldehyde.The method was applied to the determination of formaldehyde in 12 samples of iced fresh seafood.Formaldehyde was detected in 4 samples within 3.19 mg/kg-11.4 mg/kg.Conclusion The method is simple,accurate and can be used for the fast determination of formaldehyde in iced fresh seafood.